EP0015293A4 - Method and apparatus for producing hollow microspheres. - Google Patents
Method and apparatus for producing hollow microspheres.Info
- Publication number
- EP0015293A4 EP0015293A4 EP19790901239 EP79901239A EP0015293A4 EP 0015293 A4 EP0015293 A4 EP 0015293A4 EP 19790901239 EP19790901239 EP 19790901239 EP 79901239 A EP79901239 A EP 79901239A EP 0015293 A4 EP0015293 A4 EP 0015293A4
- Authority
- EP
- European Patent Office
- Prior art keywords
- microspheres
- nozzle
- blowing
- glass
- orifice
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000004005 microsphere Substances 0.000 title claims abstract description 545
- 238000000034 method Methods 0.000 title claims description 84
- 238000007664 blowing Methods 0.000 claims abstract description 321
- 239000011521 glass Substances 0.000 claims abstract description 303
- 229910052751 metal Inorganic materials 0.000 claims abstract description 198
- 239000002184 metal Substances 0.000 claims abstract description 198
- 239000006060 molten glass Substances 0.000 claims abstract description 136
- 239000012530 fluid Substances 0.000 claims abstract description 106
- 239000000203 mixture Substances 0.000 claims abstract description 101
- 239000011248 coating agent Substances 0.000 claims abstract description 88
- 238000000576 coating method Methods 0.000 claims abstract description 88
- 239000007788 liquid Substances 0.000 claims abstract description 60
- 239000007789 gas Substances 0.000 claims description 219
- 239000000463 material Substances 0.000 claims description 105
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 39
- 229910052725 zinc Inorganic materials 0.000 claims description 39
- 239000011701 zinc Substances 0.000 claims description 39
- 230000015572 biosynthetic process Effects 0.000 claims description 32
- 238000010791 quenching Methods 0.000 claims description 29
- 239000000945 filler Substances 0.000 claims description 22
- 239000006260 foam Substances 0.000 claims description 21
- 239000002923 metal particle Substances 0.000 claims description 19
- -1 organo metal compound Chemical class 0.000 claims description 19
- 239000004033 plastic Substances 0.000 claims description 18
- 229920003023 plastic Polymers 0.000 claims description 18
- KKEBXNMGHUCPEZ-UHFFFAOYSA-N 4-phenyl-1-(2-sulfanylethyl)imidazolidin-2-one Chemical compound N1C(=O)N(CCS)CC1C1=CC=CC=C1 KKEBXNMGHUCPEZ-UHFFFAOYSA-N 0.000 claims description 15
- 230000004888 barrier function Effects 0.000 claims description 15
- 239000000853 adhesive Substances 0.000 claims description 13
- 230000001070 adhesive effect Effects 0.000 claims description 13
- 238000009413 insulation Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- 239000011261 inert gas Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 230000000737 periodic effect Effects 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 239000006096 absorbing agent Substances 0.000 claims description 7
- 230000010355 oscillation Effects 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 6
- 239000004604 Blowing Agent Substances 0.000 claims description 4
- 239000010426 asphalt Substances 0.000 claims description 3
- 239000010408 film Substances 0.000 claims 33
- 239000010409 thin film Substances 0.000 claims 2
- 230000032258 transport Effects 0.000 claims 1
- 238000010276 construction Methods 0.000 abstract description 25
- 239000012774 insulation material Substances 0.000 abstract description 13
- 230000008569 process Effects 0.000 description 31
- 239000011810 insulating material Substances 0.000 description 20
- 238000004519 manufacturing process Methods 0.000 description 19
- 235000019353 potassium silicate Nutrition 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 239000002245 particle Substances 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 15
- 238000001816 cooling Methods 0.000 description 14
- 238000012546 transfer Methods 0.000 description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 239000011505 plaster Substances 0.000 description 9
- UIIMBOGNXHQVGW-UHFFFAOYSA-N sodium;hydron;carbonate Chemical compound [Na+].OC(O)=O UIIMBOGNXHQVGW-UHFFFAOYSA-N 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000000654 additive Substances 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 239000000470 constituent Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000002844 melting Methods 0.000 description 8
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 230000035699 permeability Effects 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 230000009471 action Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000006866 deterioration Effects 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
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- 239000011707 mineral Substances 0.000 description 5
- 238000010422 painting Methods 0.000 description 5
- 230000005855 radiation Effects 0.000 description 5
- 238000004513 sizing Methods 0.000 description 5
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- 229910011255 B2O3 Inorganic materials 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 4
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- 229910052759 nickel Inorganic materials 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 241000905957 Channa melasoma Species 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
- 239000003570 air Substances 0.000 description 3
- 238000004378 air conditioning Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
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- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000012809 cooling fluid Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000011152 fibreglass Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 125000000962 organic group Chemical group 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 239000011669 selenium Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- CYRMSUTZVYGINF-UHFFFAOYSA-N trichlorofluoromethane Chemical compound FC(Cl)(Cl)Cl CYRMSUTZVYGINF-UHFFFAOYSA-N 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 2
- 230000001413 cellular effect Effects 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000003203 everyday effect Effects 0.000 description 2
- 238000005247 gettering Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229920001225 polyester resin Polymers 0.000 description 2
- 229920005672 polyolefin resin Polymers 0.000 description 2
- 239000011496 polyurethane foam Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000003303 reheating Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 241001527806 Iti Species 0.000 description 1
- 241001385004 Microon Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229920002319 Poly(methyl acrylate) Polymers 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 238000009435 building construction Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 150000001728 carbonyl compounds Chemical class 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
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- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 238000010943 off-gassing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 229920006327 polystyrene foam Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
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- 230000002028 premature Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- 239000004094 surface-active agent Substances 0.000 description 1
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- 230000003313 weakening effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0072—Inorganic membrane manufacture by deposition from the gaseous phase, e.g. sputtering, CVD, PVD
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/22—Coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
- B22F1/0655—Hollow particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/0042—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor without using a mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/42—Component parts, details or accessories; Auxiliary operations
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y02E30/10—Nuclear fusion reactors
Definitions
- the present invention relates to hollow microspheres made from inorganic film forming materials and compositions and particularly to hollow glass microspheres and to a process and apparatus for making the microspheres.
- the present invention particularly relates to hollow glass vacuum microspheres -having a thin transparent metal coating deposited on the inner wall surface of the microspheres.
- a transverse jet is used to direct an inert entraining fluid over and around the blowing nozzle at an angle to the axis of the blowing nozzle.
- the entraining fluid as it passes over and around the blowing nozzle envelops and acts on the molten glass as it is being blown to form the microsphere and to detach the microsphere from the coaxial blowing nozzle.
- Quench means are disposed close to and below the blowing nozzles to direct a quench fluid onto the micro- spheres to rapidly cool and solidify the microspheres.
- the present invention also relates to a method and apparatus for making filamented glass microspheres with thin glass filaments connecting adjacent microspheres and to the filamented microspheres themselves.
- the hollow glass microspheres of the present invention are capable of withstanding relatively high external pressures and/or weight.
- Hollow glass microspheres can be made that are resistant to high temperatures and stable to many chemical agents and weathering conditions . These characteristics make the microspheres suitable for a wide variety of uses. BACKGROUND OF THE INVENTION
- filler materials utilizes hollow glass microspheres.
- the known methods for producing hollow glass microspheres for use as filler materials have not been successful in producing microspheres of uniform size or uniform thin walls which makes it very difficult to produce filler and insulation materials of controlled and predictable physical and chemical characteristics and quality.
- One of the newly developed insulation materials utilizes packed glass microspheres, the outer surface of which microspheres are coated with a reflective metal and a vacuum is maintained in the interstices area between the microspheres.
- the outer reflective metal coating minimizes heat transfer by radiation and a vacuum maintained in the interstices area minimizes heat transfer by gas conduction.
- Insulation materials, however, made from these types of micro- spheres possess several inherent disadvantages. It has been found to be difficult if not impossible in many applications to maintain the vacuum in the interstices area between the packed microspheres and loss of this vacuum increases the heat transfer by gas conduction. It has also been found very difficult and costly to deposit a relatively thin uniform film of reflective metal on the outer surface of the microspheres.
- One of the existing methods of producing hollow glass microspheres for use as insulating materials, for exa ⁇ as disclosed in the Veatch et al U.S. Patent 2,797,201 or Beck et al U.S. Patent 3.365,315 involves dispersing a liquid and/or solid gas-phase precursor material in the glass material to be blown to form the microspheres..
- the glass material con- taining the solid or liquid gas-phase precursor enclosed therein is then heated to convert the solid and/or liquid gas-phase precursor material into a gas and is further heated to expand the gas and pro- ,
- hollow glass vacuum microspheres having a reflective metal deposited on the inner wall surface thereof be used to make insu ⁇ lating materials .
- There have been several methods suggested for making this type of hollow vacuum micro ⁇ sphere but to date none of the known methods are believed to have been successful in making any such microspheres.
- the transverse jet entraining fluid can also be pulsed at regular intervals to assist in controlling the size of the microspheres and in separating the microspheres from the blowing nozzle and the distance or spacing between mico- spheres.
- the entraining fluid envelops and acts asymmetrically on the elongated cylinder and causes the cylinder to flap, fold, pinch and close-off at its inner end at a point proximate to the coaxial blowing nozzle.
- the continued movement of the entraining fluid over the elongated cylinder produces fluid drag forces on the cylinder and detaches the elongated cylinder from the coaxial blowing nozzle to have it fall free from the blowing nozzle.
- the surface tension forces of the molten glass act on the now free, entrained elongated cylinder and cause the cylinder to seek a minimum surface area and to form a spherical shape.
- Quench nozzles are disposed below and on either side of the blowing nozzle and direct cooling fluid at and into contact with the molten glass micro- spheres to rapidly cool and solidify the molten glass and form a hard, smooth hollow glass micro ⁇ sphere.
- the quench fluid cools and condenses the metal vapor and causes the metal vapor to deposit on the inner wall surface of the microsphere as a transparent metal coating or a thin reflective metal coating.
- the filamented micropsheres are made in a manner such that they are connected or attached to each other by a thin continuous glass filament.
- the filamented micro ⁇ spheres can also be flattened to produce the oblate spheroids.
- the filaments interrupt and reduce the. area of wall to wall contact between the micro ⁇ spheres and reduce the thermal conductivity between the walls of the microspheres.
- the filamented microspheres also assist in handling and preventing scattering of microspheres, particularly where very small diameter microspheres or low density microspheres are ' produced.
- the filamented micro- spheres have a distinct advantage over the simple addition of filaments in that the continuous filaments do not tend to settle in the system in which they are used.
- the inner volume of the microspheres may contain an inert low conductivity gas used to blow the microsphere or can contain a high vacuum produced by condensing a metal vapor used to blow the . microsphere.
- the hollow glass microspheres and the hollow glass vacuum microspheres of the present invention can have a transparent metal coating deposited on the inner wall surface thereof which allows sun- light to pass through the microspheres but reflects and traps infrared radiations.
- the present invention provides a method for using a metal vapor blowing gas to blow hollow glass microspheres to obtain a high contained vacuum within the microsphere.
- the present inven- tion also allows for the addition to metal vapor blowing gas small amounts of selected metal vapors, e.g. alkali metal vapors, to getter, i.e. react with trace gases that may evolve from the molten glass film as the microsphere is being formed.
- the selected metal vapors getter any evolved gases and maintain the high contained vacuum.
- the attached drawings illustrate exemplary forms of the method and apparatus of the present invention for making microspheres for use in and as insulating materials and/or for use in and as filler materials.
- the Figure 1 of the drawings shows in " cross- section an apparatus having multiple coaxial blowing nozzle means for supplying the gaseous material for blowing hollow glass microspheres, a transverse jet providing an entraining fluid to assist in the formation and detachment of the microspheres from the blowing nozzles, and means for supplying a quench fluid to cool the microspheres.
- FIG. 3a of the drawings is a detailed cross-section of a modified transverse jet entraining means having a flattened orifice opening and the Figure 3 nozzle means.
- FIG. 3b of the drawings is a top plane view of the modified transverse jet entraining means and the nozzle means illustrated in Figure 3a- of the drawings.
- FIG. 7a of the drawings shows a cross- section of oblate spheroid shaped hollow glass micro ⁇ spheres made into a formed insulation panel.
- the Figure 8 of the drawings illustrates in graphic form the relationship between the thickness of the thin metal film deposited on the inner wall surface of the hollow microsphere, the metal vapor blowing gas pressure and the diameter of the microspheres.
- the coaxial blowing nozzle 5 consists of an inner nozzle 6 having an orifice 6a for a blowing gas, an inert blowing gas or metal vapor blowing gas and an outer nozzle 7 having an orifice 7a for molten glass.
- the inner nozzle 6 is disposed within and coaxial to outer nozzle 7 to form annular space 8 between nozzles 6 and 7, which annular space provides a flow path for molten glass 2.
- the ori ⁇ fice 6a of inner nozzle 6 terminates at or a short distance above the plane of orifice 7a of outer nozzle 7.
- tubular 5 solar collector The construction and operation of the tubular 5 solar collector are otherwise essentially the same as the known tubular solar collectors .
- the constituents of the glass compositions can be selected and blended to have high resistance to corrosive gaseous materials, high resistance to gaseous chemical agents, high resistance to alkali and weather, low susceptibility to diffusion of gaseous materials into and out of the glass micro- spheres, and to be substantially free of trapped gas bubbles or dissolved gases in the walls of the microspheres which can form bubbles and to have sufficient strength when cured, hardened and solidified to support a substantial amount of weight and/or to withstand a substantial amount of pressure.
- the inert gases used to blow the microspheres are selected to have a low heat conductivity and generally involve heavy molecules which do not transfer heat readily.
- Suitable blowing gases are argon, xenon, carbon dioxide, nitrogen, nitrogen dioxide, sulfur and sulfur dioxide.
- Organo metal compounds can also be used as a blowing gas.
- the blowing gas is selected to have the desired internal pressure when cooled to ambient temperatures.
- Metal particles such as aluminum, silver, nickel, zinc, antimony, barium, cadmium, cesium, bismuth, selenium, lithium, magnesium, potassium, and gold can be used.
- Dispersed metal oxide particles can in a similar manner be used to obtain similar effects to that of the metals.
- the metal oxide particles can be used to produce a deposited film of lower heat conductivity characteristics.
- the thin metal coating can also be deposited on the inner wall surface of the microsphere by using as or with blowing gas organo metal compounds that are gases at the blowing temperatures.
- organo metal compounds that are gases at the blowing temperatures.
- the organo carbonyl compounds are preferred.
- Suitable organo metal carbonyl compounds are nickel and iron.
- the organo metal compounds can be decomposed by heating just prior to blowing the microspheres to obtain finely dispersed metal particles and a decomposition gas.
- the decomposition gas if present, can be used to assist in blowing the microspheres.
- the thickness of the deposited metal layer will depend primarily on the partial pressure of the gaseous organo metal blowing gas and the inside diameter of the microsphere.
- the blowing temperatures is molten, fluid and flows easily.
- the molten glass just prior to the blowing operation has a viscosity of 10 to 600 poises, preferably 20 to 350, and more preferably 30 to 200 poises.
- the molten lead containing glass compositions just prior to the blowing operation have a viscosity of, for example, 10 to 500 poises.
- the molten basaltic mineral glass composition just prior to the blowing operation can have a viscosity of, for example, 15 to 4(30 poises.
- the glass during the blowing operation exhibits a surface tension of 150 to 400 dynes/cm, preferably 200 to 350 dynes/cm and more preferably 250 to 325 dynes/cm.
- the molten or liquid glass fed to the coaxial blowing nozzle can be at about ambient pressure or can be at an elevated pressure.
- the molten or liquid glass feed can be at a pressure of 1 to 20,000 p.s.i.g., usually 3 to 10,000 p.s.i.g. and more usually 5 to 5,000 p.s.i.g.
- the molten glass feed when used for low pressure applications can be at a pressure of 1 to 1000 p.s.i.g., preferably 3 to 500 p.s.i.g. and more preferably 5 to 100 p.s.i.g.
- blowing gas, inert blowing gas, gaseous material blowing gas or metal vapor will be at about the same temperature as the molten glass being blown.
- the blowing gas temperature can, however, be at a higher temperature than the molten glass to assist in maintaining the fluidity of the hollow molten glass microsphere during the blowing operation or can be at a lower temperature than the molten glass to assist in the solidification and hardening of the hollow molten glass microsphere as it is formed.
- the pressure of the blowing gas is sufficient to blow the microsphere and will be slightly above the pressure of molten glass at the orifice 7a of the outer nozzle 7.
- the blowing gas pressure will also depend on and be slightly above the ambient pressure external to the blowing nozzle.
- the blowing gas or gaseous material blowing gas can also be at a pressure of 1 to 1,000 p.s.i.g., preferably 3 to 500 p.s.i.g. and more preferably 5 to 100 p.s.i.g.
- the blowing gas or gaseous material blowing gas can be at a pressure of 1 to 1,000 p.s.i.g., preferably at 3 to 100 p.s.i.g. and more preferably at 5 to 50 p.s.i.g.
- the ambient pressure external to the blowing nozzle can be at about atmospheric pressure or can be at subatmospheric or super-atmospheric pressure. Where it is desired to have a relatively or high
- the ambient pressure external to the blowing nozzle is maintained at a super- atmospheric pressure.
- the ambient pressure external to the blowing nozzle will, in any event, be such that it substantially balances, but is slightly less than the blowing gas pressure.
- pulsing the transverse jet entraining fluid at a rate of 2 to 1500 pulses/sec, preferably 50 to 1000 pulses/sec and more preferably 100 to 500 pulses/ sec assist in controlling the diameter of the micro ⁇ spheres and the length of the filament portion of the filamented microspheres and detaching the micro ⁇ spheres from the coaxial blowing nozzle.
- the distance between filamented microspheres depends to some extent on the viscosity of the glass and the linear velocity of the transverse jet entraining fluid.
- the quench fluid very rapidly cools the outer molten glass surface of the microsphere with which it is in direct contact and more slowly cools the blowing gas or metal vapor enclosed within the micro ⁇ sphere because of the lower thermal conductivity of the gas or vapor. This cooling process allows sufficient time for the glass walls of the micro ⁇ spheres to strengthenbefore the gas is cooled or the metal vapor is cooled and condensed and a high vacuum formed within the glass microsphere.
- the cooling and deposition of the metal vapor on the inner wall surface of the microspheres can be controlled to optimize the crystal size of the metal deposited such that sufficiently large crystals are obtained that the deposited metal film is discontinuous.
- the discontinuities in the metal film reduce the thermal conductivity of the metal film while at the same time retaining the metal films ability to reflect radiant heat.
- the time elapsed from commencement of the blowing of the glass microspheres to the cooling and hardening of the microspheres can be .0001 to 1.0 second, preferably .0010 to 0.50 second and more preferably 0.010 to 0.10 second.
- the process of the present invention was found to be very sensitive to the distance of the trans ⁇ verse jet 13 from the orifice 7a of outer nozzle 7, the angle at which the transverse jet was directed at coaxial blowing nozzle 5 and the point at which a line drawn through the center axis of transverse jet 13 intersected with a line drawn through the center axis of coaxial nozzle 5.
- the transverse jet 13 is aligned to direct the flow of entraining fluid 14 over and around outer nozzle 7 in the microsphere forming region of the orifice 7a.
- the orifice 13a of transverse jet 13 is located a distance of 0.5 to 14 times, preferably 1 to 10 times and more preferably 1.5 to 8 times and still more preferably 1.5 to 4 times the outside diameter of coaxial blowing nozzle 5 away from the point of intersect of a line drawn along the center axis of transverse jet 13 and a line drawn along the center axis of coaxial blowing nozzle 5.
- the center axis of transverse jet 13 is aligned at an angle of 15 to 85°, preferably 25 to 75° and more preferably 35 to
- the orifice 13a can be circular in shape and have an inside diameter of 0.32 to 0.010 inch, preferably 0.20 to 0.015 inch and more preferably 0.10 to 0.020 inch.
- the transverse jet entraining fluid as it passes over and around the blowing nozzle fluid dynamically induces a periodic pulsating or fluctu ⁇ ating pressure field at the opposite or lee side of the blowing nozzle in the wake or shadow of the coaxial blowing nozzle.
- a similar periodic pulsating or fluctuating pressure field can be produced by a pulsating sonic pressure field directed at the coaxial blowing nozzle.
- the entraining fluid assists in the formation and detaching of the hollow glass microsphere from the coaxial blowing nozzle.
- the use of the transverse jet and entraining fluid in the manner described also discourages wetting of the outer wall surface of the coaxial blowing nozzle 5 by the molten glass being blown. The wetting of the outer wall disrupts and interfers with blowing the microspheres.
- the quench nozzles 18 are disposed below and on both sides of coaxial blowing nozzle 5 a sufficient distance apart to allow the microspheres 17 to fall between the quench nozzles 18.
- the inside diameter of quench nozzle orifice 18a can be 0.1 to 0.75 inch, preferably 0.2 to 0.6 inch and more preferably 0.3 to 0.5 inch.
- the quench nozzles 18 direct cooling fluid 19 at and into contact with the molten glass microspheres 17 at a velocity of 2 to 14, preferably 3 to 10 and more preferably 4 to 8 ft/sec to rapidly cool and solidify the molten glass and form a hard, smooth -hollow glass microsphere.
- the proper gap can best be determined by pressing the. inner coaxial nozzle 6 downward with sufficient pressure to completely block-off the flow . of glass, and to then very slowly raise the inner coaxial nozzle 6 until a stable system is obtained, i.e. until the microspheres are being formed.
- the tapered nozzle construction illustrated in Figure 3 is as mentioned above the preferred embodiment of the invention.
- This embodiment can be used to blow glass compositions at relatively high viscosities as well as to blow glass compo ⁇ sitions at the relatively low viscosities referred to with regard to Figure 2 of the drawings.
- the Figure 3 embodiment of the invention is of particular advantage in blowing the thin walled microspheres for use in or as insulating materials.
- the passage of the glass material through the fine or narrow gap serves to align the additive materials with the walls of the microspheres as the micro- spheres are being formed.
- the Figures 3a and 3b of the drawings also illustrate a preferred embodiment of the invention in which the transverse jet 13 is flattened to form a generally rectangular or oval shape.
- the orifice 13a can also be flattened to form a generally oval or rectangular shape.
- the width of the orifice can be 0.96 to 0.030 inch, preferably 0.60 to 0.045 inch and more preferably 0.030 to 0.060 inch.
- the height of the orifice can be 0,32 to 0.010 inch, preferably 0.20 to 0.015 inch and more preferably 0.10 to 0.020 inch.
- the hollow microspheres made in accordance, with the present invention can be made from suitable inorganic film forming compositions.
- the compositions are preferably resistant to high temperatures and chemical attack, resistant to corrosive and alkali and resistant to weathering as the situation may require.
- compositions that can be used are those that have the necessary viscosities, as mentioned above, when being blown to form stable films and which have a rapid change from the molten or liquid state to the solid or hard state with a relatively narrow temperature chang . That is, they change from liquid to solid within a relatively narrowly defined temperature range.
- the hollow glass microspheres made in accordance with the present invention are pre ⁇ ferably made from a low heat conductivity glass composition, they are substantially uniform in diameter and wall thickness, have a clear, hard, smooth surface and are resistant to chemical attack, high temperatures and weathering.
- the hollow glass microspheres are substantially uniform in diameter and wall thickness, and depending on their composition and blowing conditions are light transparent, translucent or opaque, soft or hard, and smooth or rough.
- the wall of the microspheres are free or substantially free of any holes, relatively thinned wall portions or sections, sealing tips, trapped gas bubbles, or sufficient amounts of dissolved gases to form bubbles.
- the microspheres are also free of any latent solid or liquid blowing gas materials or gases.
- the preferred glass compositions are those that are resistant to chemical attack, elevated temperatures, weathering and diffusion of " gases into and/or out of the microspheres. Where the blowing gases may decompose at elevated temperatures, glass compositions that are liquid below the decomposition temperatures of the gases can be used.
- This procedure can in some instances also be used to optimize the metal crystal size of the deposited metal layer.
- the heat conductivity properties of the metal layer are reduced, while the radiant heat reflecting pro ⁇ perties of the metal layer are not adversely affected.
- the glass microspheres can be made in various diameters and wall thickness, depending upon the desired end use of the microspheres .
- the micro ⁇ spheres can have an outer diameter of 200 to 10,000 microns, preferably 500 to 6,000 microns and more preferably 1,000 to 4,000 microns.
- the microspheres can have a wall thickness of 0.1 to 1,000 microns, preferably 0.5 to 400 microns and more preferably 1 to 100 microns.
- the microspheres can contain a high vacuum in the enclosed volume where a metal vapor is used as a blowing gas and the metal vapor is cooled, condenses and deposits as a thin metal coating on the inner wall surface of the hollow microsphere.
- the pressure in the microsphere will be equal to the vapor pressure of the deposited metal at ambient temperature.
- the thickness of the thin metal coating depo- .ited on the inner wall surface of the microsphere will depend on the metal vapor used to blow the microspr.ere, the pressure of the metal vapor and the size of the microsphere.
- the thickness of the o thin metal coating can be 25 to 1000A, preferably
- the deposited metal coating be reflective, e.g. to o sunlight, the coating shouldobe more than 100A and preferably more than 150A thick.
- the reflective metal coated microspheres O can have a deposited metaol coating 105 to 600A and preferably 1o50 to
- the microspheres can contain a thin metal layer deposited on the inner wall surface of the microsphere where the blowing gas contains dis ⁇ persed metal particles.
- the thickness of the thin metal coating deposited on the inner wall surface of the microsphere will depend on the amount and particle size of the dispersed metal particles. or partial pressure of organo metal blowing gas that are used and the diameter of the microsphere.
- the thickness of the thin metal coating can be 25 o o to 10.000A, preferably 50 to 5.000A and more o preferably 100 to 1.000A.
- the coating should o o be less than 100A and preferably less than 80A.
- the hollow glass microspheres of the present invention can be used to design systems having superior insulating characteristics. Where only hollow microspheres are used in which the contained volume has an inert low conductivity gas, systems can be designed in which the thermal conductivity can be as low as Rll per inch, for example, R3 to Rll per inch.
- OMPI OMPI . WIPO .
- an insulating system consisting essentially of hollow glass microspheres having a low emissivity, highly reflective metal coating deposited on the inner wall surface of the microsphere and a foamed material containing a low heat conductivity gas in the interstices
- systems can be designed in which the thermal conductivity can be as low as R50 per inch, for example, R30 to R50 per inch.
- the microspheres can be used to make heat barriers by filling spaces between existing walls or other void spaces or can be made into sheets or other shaped forms by cementing the micro ⁇ spheres together with a suitable resin or other adhesive or by fusing the microspheres together and can be used in new construction.
- a glass composition comprising the following constituents is used to make hollow glass micro- spheres.
- the glass composition is heated to a tempera ⁇ ture of 2650 to 2750°F. to form a fluid molten glass having a viscosity of 35 to 60 poises and a surface tension of 275 to 325 dynes per cm.
- the molten glass is fed to the apparatus of Figures 1 and 2 of the drawings.
- the molten glass passes through annular, space 8 of blowing nozzle 5 and forms a thin liquid molten glass film across the orifices 6a and 7a.
- the blowing nozzle 5 has an outside diameter of 0.040 inch and orifice 7a
- the free falling, i.e.-entrained, elongated cylinders quickly assume a spherical shape and are rapidly cooled to about ambient temperature by a quench fluid con ⁇ sisting of a fine water spray at a temperature of 90 to 150°F. which quickly cools, solidifies and hardens the glass microspheres.
- Example 2 A glass composition comprising the following constituents is used to make transparent hollow glass vacuum microspheres.
- the glass composition is heated to a tempera ⁇ ture of 2650 to 2750°F. to form a fluid molten glass having a viscosity of 35 to 60 poises and a surface tension of 275 to 325 dynes per cm.
- the molten glass is fed to the apparatus of Figures 1 and 3 of the drawings.
- the molten glass is passed through annular space 8 of blowing nozzle 5 and into tapered portion 21 of outer nozzle 7.
- the molten glass under pressure is squeezed through a fine gap formed between the outer edge of orifice 6a and the inner surface 22 of the tapered portion 21 of outer nozzle 7 and forms a thin liquid molten glass film across the orifices 6a and 7a'.
- the blowing nozzle 5 has an outside diameter of 0.04 inch and orifice 7a' has an inside diameter of 0.01 inch.
- the thin liquid molten glass film has a diameter of 0.01 inch and a thickness of 0.003 inch.
- the transverse jet is aligned at an angle of 35 to 50° relative to the blowing nozzle and a line drawn through the center axis of the transverse jet intersects a line drawn through the center axis of the blowing nozzle 5 at a point 2 to 3 times the outside di ⁇ ameter of the coaxial blowing nozzle 5 above orifice 7a' .
- the free falling elongated cylinders filled with the zinc vapor quickly assume a spherical shape.
- the microspheres are contacted with a quench fluid consisting of a fine water spray at a temperature of 90 to 150°F. which quickly cools, solidifies and hardens the molten glass prior to cooling and condensing the zinc vapor.
- the zinc vapor begins to condense at a temperature of about 1660 to 1670°F. at which the glass composition used to make the microspheres has already began to harden and has sufficient strength not to collapse as the zinc vapor begins to and condenses on the inner wall surface of the microsphere (see Tables 2 and 3) .
- the zinc vapor condenses and deposits on the inner wall surface of the microsphere as a thin zinc metal coating.
- Clear, smooth, hollow glass microspheres having an about 800 to 900 micron diameter, a 8 to 20 micron wall thickness and having a thin o transparent zinc metal coating 85 to 95A thick
- a glass composition comprising the following constituents is used to make low emissivity, reflective hollow glass vacuum microspheres.
- the glass composition is heated to a tempera ⁇ ture of 2650 to 2750°F, to form a fluid molten glass having a viscosity of 35 to 60 poises and a surface tension of 275 to 325 dynes per cm.
- the molten glass is fed to the apparatus of Figures 1 and 3 of the drawings.
- the molten glass is passed through annular space 8 of blowing nozzle 5 and into tapered portion 21 of outer nozzle 7.
- the molten glass under pressure is squeezed through a fine gap formed between the outer edge of orifice 6a and the inner surface 22 of the tapered portion 21 of outer nozzle 7 and forms a thin liquid molten glass film across the orifices 6a and 7a' .
- the blowing nozzle 5 has an outside diameter of 0.05 inch and orifice 7a' has an inside diameter of 0.03 inch.
- the thin liquid molten glass film has a diameter of 0.03 inch and a thickness of 0.01 inch.
- An inert zinc vapor blowing gas at a temperature of 2600°F.
- the trans ⁇ verse jet is aligned at an angle of 35 to 50° re- lative to the blowing nozzle and a line drawn through the center axis of the transverse jet intersects a line drawn through the center axis of the blowing nozzle 5 at a point 2 to 3 times the outside diameter of the coaxial blowing nozzle 5 above orifice 7a' .
- the free falling elongated cylinders filled with -the zinc vapor quickly assume a spherical shape.
- the microspheres are contacted with a quench fluid consisting of an ethylene glycol spray at a temperature of 0 to 15°F. which quickly cools, solidifies and hardens the molten glass prior to cooling and condensing the zinc vapor.
- the zinc vapor begins to condense at a tempera ⁇ ture of about 1660 to 1670°F. at which the glass composition used to make the microspheres has already began to harden and has sufficient strength not to collapse as the zinc vapor begins to and condenses on the inner wall surface of the microspheres (see Tables 2 and 3) .
- the zinc vapor condenses and deposits on the inner wall surface of the microsphere as a thin zinc metal coating.
- Clear, smooth, hollow glass microspheres having an about 3000 to 4000 micron diameter, a 30 to 40 micron wall thickness and having a low emissivity, reflective zinc metal coating 325 to o
- Example 4 A glass composition comprising the following constituents is used to make low emissivity, reflective hollow glass vacuum filamented micro ⁇ spheres.
- the molten glass is fed to the apparatus of Figures 1 and 3 of the drawings under conditions similar to those used in Example 3.
- An inert zinc vapor blowing gas at a tempera ⁇ ture of 2400°F. and at a positive pressure is applied to the inner surface of the molten glass film causing the film to distend outwardly into an elongated cylinder shape with its outer end closed and its inner end attached to the outer edge of orifice 7a' .
- the transverse jet is used to direct an entraining fluid which consists of nitrogen gas at a temperature of 2400°F. at a linear velocity of 5 to 40 feet a second over and around the blowing nozzle 5 which entraining fluid assists in the formation and closing of the elongated cylinder shape and the detaching of the cylinder from the blowing nozzle while trailing a thin glass filament which is continuous with the next microsphere forming at the blowing nozzle.
- the filamented microspheres are otherwise formed in the manner illustrated and described with reference to Figure 3c of the drawings.
- the transverse jet is aligned at an angle of 35 to 50° relative to the blowing nozzle and a line drawn through the center axis of the transverse jet intersects a line drawn through the center axis of the blowing nozzle 5 at a point 2 to 3 times the outside diameter of the coaxial blowing nozzle 5 above orifice 7a' .
- the entrained elongated filamented cylinder filled with the zinc vapor assumes a spherical shape.
- the filamented microspheres are contacted with a quench fluid consisting of water spray at a temperature of . 60 to 100°F. which quickly cools, ' solidifies and hardens the molten glass prior to cooling and condensing the zinc vapor after which the zinc condenses on the inner wall surface of the microsphere.
- Clear, smooth, hollow filamented glass micro ⁇ spheres having an about 1500 to 2500 micron di ⁇ ameter, a 1.5 to 5.0 micron wall thickness and having a low emissiovity, reflective zinc metal coating 180 to 275A thick and an internal con- tained pressure of 10 " Torr are obtained.
- the lengths of the filament portions of the fila ⁇ mented microspheres is 10 to 20 times the diameter of the microspheres.
- the microspheres are closely examined and are found to be free of any entrapped bubbles and/or holes.
- the molten glass is fed to the apparatus of Figures 1 and 3 of the drawing under conditions similar to those, used in Example 3.
- a blowing gas consisting of argon and containing finely dispersed aluminum particles of 0.03 to 0.05 micron size at a temperature of 2700°F. and at a positive pressure is applied to the inner surface of the molten glass film causing the film to distend outwardly into an elongated cylinder shape with its outer end closed and its inner end attached to the outer edge of orifice 7a' .
- the transverse jet is used as before to di- recf-an' ' entraining fluid which consists of nitro ⁇ gen gas at a temperature of 2500 ⁇ F. over and around the blowing nozzle 5.
- di- recf-an' ' entraining fluid which consists of nitro ⁇ gen gas at a temperature of 2500 ⁇ F. over and around the blowing nozzle 5.
- the entrained falling elongated cylinders filled with the aR-g ' dn ' gas -containing the dis ⁇ persed aluminum particles quickly assume a spheri ⁇ cal shape.
- the microspheres are contacted with a quench fluid consisting of an ethylene glycol spray at a temperature of 0 to 15°F. which quickly cools, solidifies and hardens the molten glass. As the microspheres are further cooled and hardened, the aluminum particles deposit on the inner wall surface of the microsphere as a thin aluminum metal coating.
- the area between the outer cover and the upper surface of the black coated metal absorber plate is filled to a depth of about one inch with transparent glass vacuum microspheres made by the method of Example 2 of about 800 micron diameter, 10 micron wall thickness and haviong a thin transparent zinc metal coating about 85A thick and an internal
- the area between the lower surface of the black coated metal absorber plate and the inner cover member is filled to a depth of about 1 1/2 inches with the reflective glass vacuum micro- spheres made by the method of Example 3 of about
- Example 7 An efficient tubular solar energy collector, as illustrated in Figure 6 of the drawings , is constructed using the glass vacuum microspheres of the present invention as a superior insulating material.
- a tubular solar collector six feet in length and about 4 1/4 inches in diameter is con ⁇ structed.
- the outer cover consists of a clear glass or weather resistant plastic 1/8 inch thick.
- the two parallel sides and the lower curved por ⁇ tion are constructed from metal or plastic about 1/8 inch thick.
- the lower curved portion is coated with a highly reflective surface for reflecting and concentrating the sun's rays towards the center of the tubular collector.
- the tubular collector has end members closing the
- the inner feed tube is coaxial to the outer return tube.
- the outer return tube has on its outer surface a black heat absorbing coating of the type described in Example 6.
- the inner feed tube can be one inch in diameter and the outer return tube can be two inches in diameter.
- the tubular collectors are normally mounted in parallel in a manner such that they intercept the movement of the sun across the sky.
- the area between the outer cover, the sides and the lower curved portion and the double pipe tubular member is filled with transparent glass vacuum microspheres made by the method of Example 2 to provide an about one inch layer of transparent vacuum microspheres completely around the double pipe tubular member.
- the transparent glass vacuum microspheres are 800 microns in diameter, have a wall thickness of 10 microons and a thin transparent zinc metal coating 85A thick and contain an internal pres- sure. of l ⁇ "6 Torr.
- the tubular solar energy collector has a suitable inlet and outlet means for a water heat exchange medium. On a bright sunny day with an outside temperature of 90°F. , it is found that inlet water at a temperature of 80°F. , on a single
- O pass is heated to an outlet temperature of 240°F.
- An outlet temperature of 240°F. is more than suffi ⁇ cient for summer air-conditioning needs .
- the same tubular solar energy collector on a bright sunny day with an outside temperature of 32°F. it is found that inlet water at a temperature of 80°F. is heated to an outlet temperature of 170°F.
- An outlet temperature of 170°F. is more than sufficient for winter household heating and hot water require- ents.
- the Figure 7 of the drawings illustrates the use of the hollow glass microspheres of the pre ⁇ sent invention in the construction of a one-inch thick formed wall panel.
- the wall panel contains, multiple layers of uniform size glass microspheres made by the method of Example 4 of the invention.
- the microspheres have a 1500 to 2500, e.g. 2000, micron diameter, 1.5 to 5.0, e.g. 2.0, micron wall thickness ando a thino, low emissiovity zinc metal coating 180A to 275A, e.g. 250A, thick deposited on the inner wall surface of the microsphere and an internal contained pressure of 10 ⁇ Torr.
- the interstices between the microspheres is filled with low heat conductivity foam containing Freon-11 gas.
- the microspheres are treated with a thin adhesive coating and formed into a 7/8 inch thick layer.
- the adhesive is allowed to cure to form a semi-rigid wall board.
- the facing surface of the wall board is coated with an about 1/8 inch thick.plaster which is suitable for subsequent sizing and painting and/or covering with wall paper.
- the backing surface of the panel is coated with an about 1/16 inch coating of a suitable plastic composition to form a vapor seal.
- the final panels are allowed to cure.
- the cured panels form strong wall.panels which can be sawed and nailed and readily used in construction of new homes. Several sections of the panels are tested and found to have a R value of 30 per inch.
- a low heat con ⁇ ductivity resin adhesive foam containing Freon-11 gas is mixed with the microspheres and formed into a layer one-inch thick and pressed and flattened between two flat plates to form the microspheres into an oblate spheroid shape in which the ratio of the height to length of the flattened microspheres is about 1:3.
- the flattened micro ⁇ spheres are held in this position until the adhesive foam resin surrounding the microspheres cures after which microspheres retain their flattened shape.
- the interstices between the microspheres - are thus filled with a low heat-conductivity foam containing Freon-11 gas.
- the facing surface of the wall board is about 1/8 inch plaster which is suitable for subsequent sizing and painting and/or covering with wall paper.
- the backing of the wall panel is about a 1/16 inch coating of plastic which forms a vapor seal.
- the panels are cured and form strong wall panels which can be sawed and nailed and readily used in construction of new homes. Several sections of the panel are tested and found- to have a R value of 50 per inch.
- the density of the back one-third of the panel can be about one-half to one-third that of the center third of the panel.
- the sides of the panel can be reversed, i.e. the high density side can face outward.
- the hollow glass microspheres of the present invention have many uses including the manufacture of superior insulating materials and the use of the microspheres as a filler or aggregate in cement, plaster and asphalt and synthetic con ⁇ struction board materials.
- the microspheres can also be used in the manufacture of insulated -louvers and molded objects or forms.
- the microsphere can be used to form thermal insulation barriers merely by filling spaces be ⁇ tween the walls of refrigerator trucks or train cars, household refrigerators, cold storage building facilities, homes, factories and office buildings.
- the microspheres may be adhered together with known adhesives or binders to produce semi- or rigid cellular type materials for use in manu ⁇ facturing various products or in construction.
- the microspheres because they are made from very stable glass compositions, are not subject to degradation by outgassing, aging, moisture, weathering or biological attack and do not produce toxic fumes when exposed to very high temperatures or fire.
- the hollow .glass micro ⁇ spheres when used in manufacture of superior insulating materials can advantageously be used alone or in combination with fiberglass, styro- foam, polyurethane foam, phenol-formaldehyde foam, organic and inorganic binders and the like.
- the gases can be encapsulated in very durable alumina silicate or zirconia glass microspheres which can subsequently be embedded, if desired, in a con ⁇ crete structure.
- the glass microspheres of the present invention because they can be made to contain gases under high pressure, can be used to manufacture fuel targets for laser fusion reactor systems.
- the process and apparatus of the invention can also be used to form hollow microspheres from - metals such as iron, steel, nickel, gold, copper, zinc, tin, brass, lead, aluminum and magnesium.
- suitable, additives are used which provide at the surface of a blown microsphere a sufficiently high viscosity that a stable microsphere can be formed.
- the process of the present invention can also be carried out in a centrifuge apparatus in which the coaxial blowing nozzles are disposed in the outer circumferal surface of the centrifuge.
- Liquid glass is fed into the centrifuge and because of centrifugal forces rapidly coats and wets the inner wall surface of the outer wall of the centrifuge,
- the liquid glass is fed into the outer coaxial nozzle.
- the inlet to the inner coaxial nozzle is disposed above the coating of liquid glass.
- the blowing gas is as before fed into the inner coaxial nozzle.
- the transverse jet entraining fluid is provided by transverse jets mounted on the outer surface of the rotating bowl.
- An external gas can be directed along the longi ⁇ tudinal axis of the centrifuge to assist in removing the microspheres from the vicinity of the .centrifuge as they are formed. Quench, fluids can be provided as before.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Structural Engineering (AREA)
- Thermal Sciences (AREA)
- Sustainable Energy (AREA)
- Power Engineering (AREA)
- Sustainable Development (AREA)
- Civil Engineering (AREA)
- Nanotechnology (AREA)
- Electromagnetism (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Computer Hardware Design (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Ocean & Marine Engineering (AREA)
- Composite Materials (AREA)
- Plasma & Fusion (AREA)
- High Energy & Nuclear Physics (AREA)
- Glass Compositions (AREA)
- Surface Treatment Of Glass (AREA)
- Joining Of Glass To Other Materials (AREA)
- Laminated Bodies (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
Description
Claims
Applications Claiming Priority (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US93712378A | 1978-08-28 | 1978-08-28 | |
US937123 | 1978-08-28 | ||
US94464378A | 1978-09-21 | 1978-09-21 | |
US944643 | 1978-09-21 | ||
US5929779A | 1979-07-20 | 1979-07-20 | |
US59297 | 1979-07-20 |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP82110062.5 Division-Into | 1982-11-01 | ||
EP86114167.9 Division-Into | 1986-10-13 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0015293A1 EP0015293A1 (en) | 1980-09-17 |
EP0015293A4 true EP0015293A4 (en) | 1981-06-30 |
EP0015293B1 EP0015293B1 (en) | 1985-07-03 |
Family
ID=27369620
Family Applications (4)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP86114167A Expired EP0226738B1 (en) | 1978-08-28 | 1979-08-17 | Filamented, hollow microspheres and applications thereof |
EP82110062A Expired EP0080078B1 (en) | 1978-08-28 | 1979-08-17 | Hollow microspheres and applications thereof |
EP79901239A Expired EP0015293B1 (en) | 1978-08-28 | 1980-03-25 | Method and apparatus for producing hollow microspheres |
EP79901171A Withdrawn EP0016818A1 (en) | 1978-08-28 | 1980-03-25 | Method for compressing gaseous materials in a contained volume |
Family Applications Before (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP86114167A Expired EP0226738B1 (en) | 1978-08-28 | 1979-08-17 | Filamented, hollow microspheres and applications thereof |
EP82110062A Expired EP0080078B1 (en) | 1978-08-28 | 1979-08-17 | Hollow microspheres and applications thereof |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP79901171A Withdrawn EP0016818A1 (en) | 1978-08-28 | 1980-03-25 | Method for compressing gaseous materials in a contained volume |
Country Status (6)
Country | Link |
---|---|
EP (4) | EP0226738B1 (en) |
JP (3) | JPS6253221B2 (en) |
CA (2) | CA1149170A (en) |
DE (2) | DE2950447A1 (en) |
GB (6) | GB2048847B (en) |
WO (2) | WO1980000438A1 (en) |
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EP0226738B1 (en) * | 1978-08-28 | 1989-06-14 | TOROBIN, Leonard B. | Filamented, hollow microspheres and applications thereof |
US4415512A (en) * | 1979-07-20 | 1983-11-15 | Torobin Leonard B | Method and apparatus for producing hollow metal microspheres and microspheroids |
US4363646A (en) * | 1979-07-20 | 1982-12-14 | Torobin Leonard B | Method and apparatus for producing microfilaments |
GB2139616B (en) * | 1983-05-13 | 1987-04-01 | Glaverbel | Gas-filled glass beads |
GB2225426B (en) * | 1988-09-29 | 1993-05-26 | Michael John Gill | A transducer |
GB2246349B (en) * | 1990-07-24 | 1994-06-22 | British Gas Plc | Method for bonding together hollow glass spheres |
GB2249088A (en) * | 1990-10-03 | 1992-04-29 | Shearn Matthew Bruce | Hollow sphere or foam containing an internal coating and vacuum |
GR1001255B (en) * | 1990-10-15 | 1993-06-30 | Glaverbel | Glazed enamel preparations |
DE4120764C1 (en) * | 1991-06-24 | 1992-06-04 | Frank 8911 Eresing De Martiny | |
DE19519984A1 (en) * | 1995-05-24 | 1996-11-28 | Ulrich Kasperek | Thermal insulation layer for vehicles, buildings, machinery or over garments |
GB2323282B (en) | 1997-03-17 | 2001-03-07 | Bristol Myers Squibb Co | Improvements relating to hygiene and medical products |
KR20000000997A (en) * | 1998-06-05 | 2000-01-15 | 이재흥 | Mobile drilling device |
DE19849135A1 (en) * | 1998-10-23 | 2000-04-27 | D.D.C. Planungs-, Entwicklungs- Und Management Ag | Polyurethane foam-based building material contains foliated glass as mineral filler added during the preparation but prior to foaming |
GB2354571A (en) * | 1999-09-23 | 2001-03-28 | Cavan Frederick Edward Adolphe | Insulation having a partial or total vacuum |
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US7794805B2 (en) * | 2007-06-29 | 2010-09-14 | Schlumberger Technology Corporation | Thermal insulation barriers |
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CN103972551A (en) * | 2014-04-03 | 2014-08-06 | 上海华篷防爆科技有限公司 | Power generating device provided with stainless steel hydrogen storage device |
US10330394B2 (en) | 2017-06-16 | 2019-06-25 | Ford Global Technologies, Llc | Heat transfer mediums |
CN115997083A (en) * | 2020-07-14 | 2023-04-21 | 国立研究开发法人物质·材料研究机构 | Mixed aerogel, method for producing same, and heat insulating material using mixed aerogel |
JPWO2022107365A1 (en) * | 2020-11-20 | 2022-05-27 |
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-
1979
- 1979-08-17 EP EP86114167A patent/EP0226738B1/en not_active Expired
- 1979-08-17 GB GB7943901A patent/GB2048847B/en not_active Expired
- 1979-08-17 WO PCT/US1979/000621 patent/WO1980000438A1/en unknown
- 1979-08-17 DE DE792950447A patent/DE2950447A1/en active Granted
- 1979-08-17 JP JP54501581A patent/JPS6253221B2/ja not_active Expired
- 1979-08-17 EP EP82110062A patent/EP0080078B1/en not_active Expired
- 1979-08-17 DE DE2954563A patent/DE2954563C2/de not_active Expired - Lifetime
- 1979-08-24 WO PCT/US1979/000651 patent/WO1980000439A1/en unknown
- 1979-08-24 GB GB7943903A patent/GB2050345B/en not_active Expired
- 1979-08-27 CA CA000334618A patent/CA1149170A/en not_active Expired
-
1980
- 1980-03-25 EP EP79901239A patent/EP0015293B1/en not_active Expired
- 1980-03-25 EP EP79901171A patent/EP0016818A1/en not_active Withdrawn
-
1982
- 1982-06-22 GB GB08218104A patent/GB2112923B/en not_active Expired
- 1982-06-22 GB GB08218037A patent/GB2112769B/en not_active Expired
- 1982-06-22 GB GB08218038A patent/GB2113668B/en not_active Expired
- 1982-07-05 GB GB08219361A patent/GB2111971B/en not_active Expired
-
1983
- 1983-02-22 CA CA000422148A patent/CA1171284A/en not_active Expired
-
1989
- 1989-09-30 JP JP1253800A patent/JPH02258650A/en active Granted
-
1990
- 1990-04-06 JP JP2090484A patent/JPH03115130A/en active Granted
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2452600A1 (en) * | 1974-11-06 | 1976-05-13 | Helmut Lehle | Tubes with metallised bores, esp optical fibres - obtd by feeding metal wire into the bore when drawing the fibre |
Also Published As
Publication number | Publication date |
---|---|
WO1980000439A1 (en) | 1980-03-20 |
GB2113668A (en) | 1983-08-10 |
DE2950447A1 (en) | 1981-01-15 |
EP0226738A1 (en) | 1987-07-01 |
GB2112769B (en) | 1983-11-16 |
JPH0324413B2 (en) | 1991-04-03 |
JPH02258650A (en) | 1990-10-19 |
JPS55500614A (en) | 1980-09-04 |
GB2111971B (en) | 1983-11-30 |
JPH03115130A (en) | 1991-05-16 |
GB2112923B (en) | 1983-11-30 |
GB2050345B (en) | 1983-06-15 |
EP0015293B1 (en) | 1985-07-03 |
EP0080078B1 (en) | 1987-07-29 |
GB2113668B (en) | 1984-02-15 |
EP0226738B1 (en) | 1989-06-14 |
EP0016818A1 (en) | 1980-10-15 |
EP0015293A1 (en) | 1980-09-17 |
JPS6253221B2 (en) | 1987-11-09 |
GB2111971A (en) | 1983-07-13 |
GB2048847A (en) | 1980-12-17 |
CA1171284A (en) | 1984-07-24 |
GB2112923A (en) | 1983-07-27 |
WO1980000438A1 (en) | 1980-03-20 |
GB2112769A (en) | 1983-07-27 |
GB2048847B (en) | 1983-07-06 |
EP0080078A3 (en) | 1983-09-07 |
DE2954563C2 (en) | 1990-09-20 |
CA1149170A (en) | 1983-07-05 |
JPH0446910B2 (en) | 1992-07-31 |
GB2050345A (en) | 1981-01-07 |
DE2950447C2 (en) | 1991-08-01 |
EP0080078A2 (en) | 1983-06-01 |
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